Many materials are made up of small crystals, or grains. Grain boundaries are the interfaces between two grains and affect the flow of heat through the material. These interfaces serve to interfere with the energy carriers by scattering or disrupting them. Because of the negative effect these interfaces have on these energy carriers, they inhibit heat flow and act as thermal resistors. The thermal boundary resistance between two grains of the same material is sometimes referred to as the Kapitza resistance, although this term is also used to describe the thermal resistance between solid/solid interfaces of different materials or solid/liquid interfaces. A better understanding of the heat transport process on a micro-scale is especially relevant to nuclear energy applications. Nuclear fuels are polycrystalline materials that experience large heat differences over small distances. An improved understanding of these grain boundaries and the role they play in transferring heat can help better predict nuclear fuel performance and improve nuclear reactor efficiency and safety. The study of the thermal resistance across crystal interfaces and their potential influence on nuclear fuels is a topic that has received relatively little attention. While the thermal resistance across a single grain boundary is rather small, the total resistance generated from many grain boundaries can have a big impact on the material. Smaller grains mean there are more interfaces, which will result in a lower overall thermal conductivity. For this study, Kapitza resistance across individual grain boundaries was measured using a laser-based measurement technique. The sample material was Cerium Oxide. It was used because of its similar properties to Uranium Oxide, which is a popular material used in nuclear fuel. The average interfacial thermal resistance measured at room temperature in this thesis study was 9.88∙10-9 �2�/�. The average measured value fit in an accepted range from other results found in similar studies.

Les matériaux à changement de phase (PCM) sont utilisés pour la réalisation de mémoire non volatile. Ces matériaux possèdent la particularité de passer d’un état cristallin à un état amorphe à l’aide d’une impulsion de chaleur, créant ainsi un processus propre au stockage de l’information. Les PCMs sont généralement basés sur des composés ternaires de type Ge-Sb-Te (GST) avec une température de transition de l’ordre de 125°C, rendent ces matériaux inutilisable dans le domaine de l’automobile et pour des applications militaires. Pour contourner cette limitation, le GST est remplacé par le composé In-Sb-Te (IST) possèdent une température de transition plus élevé et un temps de transition beaucoup plus rapide (nanoseconde). Les propriétés thermiques de l’IST et de ses interfaces au sein de la cellule PCM peuvent influencer la température de transition. C’est pourquoi la mesure de la conductivité thermique nous donnera une estimation de la valeur de cette transition.Différentes techniques ont été misent en oeuvre pour mesurer la conductivité thermique des couches minces d’IST en fonction de la concentration en Te, à savoir ; la radiométrie photo-thermique modulée (MPTR) et la méthode 3ω dans une gamme de température allant de l’ambiant jusqu'à 550°C.Les résultats obtenus par les deux techniques de caractérisation thermiques démontrent que la conductivité thermique de l'IST diminue lorsque l'on augmente la teneur en Te. L'augmentation de la teneur en Te pourrait donc conduire à un alliage thermiquement plus résistif, qui est censé apporter l'avantage d'un flux de chaleur plus confiné et limiter la cross-talk thermique dans le dispositif de mémoire à changement de phase. / Phase change memories (PCM) are typically based on compounds of the Ge-Sb-Te (GST) ternary system. Nevertheless, a major drawback of PCM devices is the failure to fulfill automotive-level or military-grade requirements (125°C continuous operation), due to the low crystallization temperature of GST. To overcome this limitation, alloys belonging to the In-Sb-Te (IST) system have been proposed, which have demonstrated high crystallization temperature, and fast switching. Thermal properties of the chalcogenide alloy and of its interfaces within the PCM cell can influence the programming current, reliability and optimized scaling of PCM devices. The two methods, namely: 3ω and Modulated Photothermal Radiometry (MPTR) technique was implemented to measure the thermal conductivity of IST thin films as well as the thermal boundary resistance at the interface with other surrounding materials (a metal and a dielectric). The experiment was carried outin situ from room temperature up to 550oC in order to investigate the intrinsic thermal properties at different temperatures and the significant structural rearrangement upon the phase transition.The results obtained from the two thermal characterization techniques demonstrate that the thermal conductivity of IST decreases when increasing the Te content. Increasing the Te content could thus lead to a more thermally resistive alloy, which is expected to bring the advantage of a more confined heat flow and limiting the thermal cross-talk in the phase change memory device.

Avec la miniaturisation croissante des systèmes micro et nanoélectroniques, les problématiques thermiques revêtent un enjeu croissant. En effet, la faible taille des composants rend problématique l'évacuation de chaleur. Selon la NASA, 90% des défaillances sont imputables à des défauts d'interconnections thermiques et d'après l'US Air Force, 55% des défaillances électroniques sont attribuables à des effets thermiques. Devenues très courantes dans les domaines des nanotechnologies et des énergies renouvelables, les couches minces présentent des caractéristiques thermiques propres (confinement) et des défis métrologiques particuliers (taille des échantillons, influence du substrat sur la mesure). Le transfert de chaleur à l'échelle submicrométrique diffère du transfert de chaleur dans les matériaux massifs à cause de l'effet de confinement spatial propre aux nanostructures. Ainsi, la diffusivité thermique α et la conductivité thermique κ de ces couches minces sont des paramètres qui affectent la performance et la durée de vie de ces couches dans une application donnée. Ce mémoire de thèse porte sur le développement d'un banc de mesure, basé sur les variations de réflectivité d'un matériau en fonction de la température ou thermoréflectance, pour la caractérisation thermique à l'échelle submicrométrique. Dans ce travail, nous avons développé des modèles thermiques tridimensionnels dans des systèmes à deux et trois couches ainsi que les expressions théoriques du signal de thermoréflectance mesuré suite à une excitation thermique de la surface de l'échantillon. Ces expressions ont été développées en tenant compte de l'effet des résistances thermiques aux interfaces. Les modèles ont été validés expérimentalement par des mesures sur des couches minces d'or déposées sur un substrat de silice. Les mesures de thermoréflectance ont été ensuite appliquées à des couches minces d'acide polylactique. Finalement, des couches minces d'oxyde de zinc dopées par différentes concentrations d'aluminium ont été élaborées par voie électrochimique et leurs propriétés thermiques étudiées à l'aide du banc de mesure de thermoréflectance. / With the increasing miniaturization of micro and nanoelectronic systems, the thermal behavior of these systems has become more and more important. The small size of the components makes the heat emitted more troublesome. According to NASA, 90% of failures are due to thermal interconnection faults and according to the US Air Force, 55% of electronic failures are attribuable to thermal effects. Most electronic chips are manufactured using thin films technologies ; therefore, the characteristics of thin metal films have been the bottom line in the ongoing research in nanotechnology and renewable energy domain. Nanoscale heat transfer is different from the heat transfer in bulk materials due to the spatial confinement effect specific to nanostructures. Furthermore, the thermal diffusivity α and thermal conductivity κ of these films are critical parameters affecting their performance and lifetime in a given application. This thesis is devoted to setting up a measurement bench, based on the reflectivity variations of a material as a function of temperature (thermoreflectance), in order to thermally characterize thin films. In this work, a three-dimensional theoretical model is developed in order to describe the temperature distribution in two and three layers systems and obtain the expression of the measured thermoreflectance signal when the surface of the sample is heated by an intensity-modulated Gaussian laser beam. These expressions are obtained by taking into consideration the effect of thermal boundary resistances. These models have been validated experimentally on thin films of gold deposited on fused silica substrate. The thermoreflectance measurements have been then performed on thin films of polylactic acid. Finally, thin films of zinc oxide doped with different concentrations of aluminum have been elaborated during this thesis. The thermal characterization of these films is carried out with the thermoreflectance bench.

La caractérisation thermique est cruciale pour la conception et le développement d'applications critiques dans divers domaines. Elle trouve son utilisation dans la détection de défauts et de points chauds dans la fabrication de semi-conducteurs, l'imagerie sous-sol ainsi que la recherche de transport thermique et de charge à des longueurs inférieures à 100 nm. La capacité de comprendre et de contrôler les propriétés thermiques des nanostructures à un niveau de sous-micron est essentielle pour obtenir les performances souhaitées. Pour atteindre cet objectif, la microscopie thermique à balayage (SThM) est très bien adaptée pour cartographier la conductivité thermique à la surface des matériaux et des appareils à l'échelle nanométrique.SThM est une technique d'imagerie "champ proche". C'est une méthode de contact, la sondeétant en contact avec la surface à une force contrôlée. STHM utilise une structure cantilever identique à celle des sondes utilisées dans un Microscope à Force Atomique (AFM). La principale différence est le fait qu'un capteur thermique est intégré à la pointe de la sonde. En outre, ce capteur peut également être utilisé comme chauffage dans le cas d'éléments thermorésistants tels que Pt ou Pd. Par conséquent, le SThM est le résultat d'un AFM équipé d'une sonde thermique. Cet instrument fournit une résolution sous-micromètre dans la résolution spatiale, c'est-à-dire plus que la résolution des techniques optiques dans la gamme de longueurs d'onde visible. La résolution classique qui est réalisée de nos jours est de l'ordre de moins de 100nanomètres alors que celle obtenue avec la première sonde Wollaston était environ 10 fois plus élevée.Par conséquent, mesurer la température et les propriétés thermiques de la matière à la microscales ont deux objectifs difficiles qui ont monopolisé l'énergie et le temps de nombreux chercheurs partout dans le monde depuis plusieurs décennies. Ces deux objectifs ne sont pas similaires. Tout d'abord, la mesure d'une température dans un domaine dont la dimension caractéristique est inférieure au micromètre semble moins difficile que mesurer la conductivité thermique d'un matériau à cette échelle. [...] / The objective of this thesis is to master quantitative aspects when using nearfield thermal microscopy by using the scanning thermal microscopy technique (SThM). We start by taking an in-depth look into the work performed previously by other scientist and research organizations. From there, we understand the progress the SThM probes have made through the decades, understand the probe sensitivity to the range of conductivity of the materials under investigation, verify the resistances encountered when the probe comes in contact with the sampl and the applications of SThM.Then we look into the equipment necessary for performing tests to characterize material thermal properties. The SThM we use is based on atomic force microscope (AFM) with a thermal probe attached at the end. The AFM is described in this work along with the probes we have utilized.For the purpose of our work, we are only using thermoresistive probes that play the role of the heater and the thermometer. These probes allow us to obtain sample temperature and thermalconductivity. We use two different types of thermal probes – 2-point probe and 4-point probe with SiO2 or with Si3N4 cantilever. Both the probes are very similar when it comes to functioning with the major difference being that the 4-point probe doesn’t have current limiters. Then, we present the use of recent heat-resistive probes allowing to reach a spatial resolution of the orde rof 100 nm under atmosphere and of 30 nm under vacuum. These probes can be used in passive mode for measuring the temperature at the surface of a material or component and in activemode for the determination of the thermal properties of these systems. Using thermoresistive probes means that no specialized devices are necessary for operation. Using simple commercialsolutions like simple AC or DC current and Wheatstone bridge are sufficient to provide basic thermal images. In our case we have also utilized other industrial devices and a home madeSThM setup to further improve the quality of measurement and accuracy. All the elements of the experimental setup have been connected using GPIB and that have been remotely controlled from a computer using a code developed under Python language. This code allows to make the frequency dependent measurement as well as the probe calibration. [...]

The Antimatter Experiment: Gravity, Interferometry, Spectroscopy (AEGIS) at the European Organization for Nuclear Research (CERN) is an experiment investigating the influence of earth’s gravitational force upon antimatter. To perform precise measurements the antimatter needs to be cooled to a temperature of 100 mK. This will be done in a Penning trap, formed by several electrodes, which are charged with several kV and have to be individually electrically insulated. The trap is thermally linked to a mixing chamber of a 3He-4He dilution refrigerator. Two link designs are examined, the Rod design and the Sandwich design. The Rod design electrically connects a single electrode with a heat exchanger, immersed in the helium of the mixing chamber, by a copper pin. An alumina ring and the helium electrically insulate the Rod design. The Sandwich uses an electrically insulating sapphire plate sandwiched between the electrode and the mixing chamber. Indium layers on the sapphire plate are applied to improve the thermal contact. Four differently prepared test Sandwiches are investigated. They differ in the sapphire surface roughness and in the application method of the indium layers. Measurements with static and sinusoidal heat loads are performed to uncover the behavior of the thermal boundary resistances. The thermal total resistance of the best Sandwich shows a temperature dependency of T-2,64 and is significantly lower, with roughly 30 cm2K4/W at 50 mK, than experimental data found in the literature. The estimated thermal boundary resistance between indium and sapphire agrees very well with the value of the acoustic mismatch theory at low temperatures. In both designs, homemade heat exchangers are integrated to transfer the heat to the cold helium. These heat exchangers are based on sintered structures to increase the heat transferring surface and to overcome the significant influence of the thermal resistance (Kapitza resistance). The heat exchangers are optimized concerning the adherence of the sinter to the substrate and its sinter height, e.g. its thermal penetration length. Ruthenium oxide metallic resistors (RuO2) are used as temperature sensors for the investigations. They consist of various materials, which affect the reproducibility. The sensor conditioning and the resulting good reproducibility is discussed as well.

The Antimatter Experiment: Gravity, Interferometry, Spectroscopy (AEGIS) at the European Organization for Nuclear Research (CERN) is an experiment investigating the influence of earth’s gravitational force upon antimatter. To perform precise measurements the antimatter needs to be cooled to a temperature of 100 mK. This will be done in a Penning trap, formed by several electrodes, which are charged with several kV and have to be individually electrically insulated. The trap is thermally linked to a mixing chamber of a 3He-4He dilution refrigerator. Two link designs are examined, the Rod design and the Sandwich design. The Rod design electrically connects a single electrode with a heat exchanger, immersed in the helium of the mixing chamber, by a copper pin. An alumina ring and the helium electrically insulate the Rod design. The Sandwich uses an electrically insulating sapphire plate sandwiched between the electrode and the mixing chamber. Indium layers on the sapphire plate are applied to improve the thermal contact. Four differently prepared test Sandwiches are investigated. They differ in the sapphire surface roughness and in the application method of the indium layers. Measurements with static and sinusoidal heat loads are performed to uncover the behavior of the thermal boundary resistances. The thermal total resistance of the best Sandwich shows a temperature dependency of T-2,64 and is significantly lower, with roughly 30 cm2K4/W at 50 mK, than experimental data found in the literature. The estimated thermal boundary resistance between indium and sapphire agrees very well with the value of the acoustic mismatch theory at low temperatures. In both designs, homemade heat exchangers are integrated to transfer the heat to the cold helium. These heat exchangers are based on sintered structures to increase the heat transferring surface and to overcome the significant influence of the thermal resistance (Kapitza resistance). The heat exchangers are optimized concerning the adherence of the sinter to the substrate and its sinter height, e.g. its thermal penetration length. Ruthenium oxide metallic resistors (RuO2) are used as temperature sensors for the investigations. They consist of various materials, which affect the reproducibility. The sensor conditioning and the resulting good reproducibility is discussed as well.